Thermal insulating foamy geopolymers from perlite

V. Vaou, D. Panias
*
Laboratory of Metallurgy, School of Mining and Metallurgical Engineering, National Technical University of Athens, Athens, Greece
a r t i c l e i n f o
Article history:
Received 10 June 2010
Accepted 27 July 2010
Keywords:
Geopolymers
Perlite
Thermal insulation
Inorganic foams
a b s t r a c t
Geopolymerization is an emerging technology which utilizes solid aluminosilicate raw materials that are
easily soluble in caustic solutions, in order to produce inorganic polymers with excellent physical,
mechanical and thermal properties. In this paper is demonstrated the ability of geopolymerization tech-
nology for production of thermal insulating foamy inorganic polymers utilizing as solid raw material
ultrane perlite which is a by-product from comminution and sizing operations of perlite exploitation.
Hydrogen peroxide is used as a chemical blowing agent for the foaming of inorganic polymers. The effect
of addition of the blowing agent on the thermophysical properties of thermal insulating materials is dem-
onstrated and these properties are compared with the ones of the commercial thermal insulating mate-
rials indicating the high potentiality for the development of this new family of inorganic polymeric
materials.
2010 Elsevier Ltd. All rights reserved.
1. Introduction
The energy consumption in the sectors of households and ser-
vices for the European Union of 27 member states amounted
388.46 Mtoe in 1990 and increased further to 455.18 Mtoe in
2006, whichconstitutes anincrease of 17%(EUenergyandtransport,
2009). The major part of this consumption is attributed to the build-
ings heating, ventilation and air-conditioning. The gures in the
north European Mediterranean countries are even worse. For the
same time period, the increase in energy consumptionin the sectors
of households andservices was 101.6%inGreece, 93%inSpain, 86.5%
in Portugal, 184.2% in Cyprus, 30.6% in Italy and 16.66% in Malta (EU
energy and transport, 2009). In order to invert this trend in energy
consumption, EU adopted specic legislation on the energy perfor-
mance of buildings (Directives 2002/91/EC, 2005/32/EC and 2006/
32/EC), which is a cost effective way of improving energy security
and ghting against climate change. In this environment, the princi-
ples of bioclimatic design and thermal insulation in buildings
(Giama and Papadopoulos, 2007) grew up and became basic design
tools for the sector of building construction.
The most important thermal insulating materials for buildings
(Karamanos et al., 2005) are classied in two categories; (a) organ-
ic and (b) inorganic materials. The European market of organic
materials is dominated by the foamy polystyrene products ex-
truded polystyrene (XPS) and Expanded Polystyrene (EPS). The
most widely used inorganic materials are the brous glass wool
and stone wool which belong to the same group of mineral wool.
Although both organic and inorganic materials are good insulating
materials they have a number of technical limitations. Polystyrene
is highly ammable or easily ignited and is classied as a B2 or B3
product according to DIN4102. When polystyrene is burned
(Department of Energy 1; Department of Energy 2; Hawley et al.,
1984) at high temperatures (800900 C) or at lower temperatures
(as in case of household replace or in a campre) polycyclic
aromatic hydrocarbons (PAHs) can be produced creating serious
health effects. Although the available re-retardant grades are
inammable, they could possibly create health and environmental
risks due to the use of brominated ame retardants such as hexa-
bromocyclododecane (EPA, 2008). Expanded polystyrene breaks
down gradually when exposed to direct sunlight or to tempera-
tures higher than 80 C and reacts with common solvents (Bynum,
2001; Papadopoulos, 2005; Al-Homoud, 2005). The blowing agent
for the production of EPS is usually pentane which may pose a
ammability hazard in manufacturing and storage of new prod-
ucts. Carbon dioxide or hydrochlorouorocarbons (HCFCs) are used
as propellant gases for the production of XPS having obvious
effects on ozone depletion and global warming (Papadopoulos,
2005). Finally, the maximum temperature at which polystyrene
products can be exposed without losing their thermophysical
properties is 7580 C (Papadopoulos, 2005). Mineral wool insula-
tion is cheaper than the organic ones and is non-ammable classi-
ed as an A1 or A2 product according to DIN4102 (Papadopoulos,
2005; Karamanos et al., 2005). In addition, it can withstand very
high temperatures (500750 C) without losing its thermophysical
properties (Papadopoulos, 2005). Two are the main drawbacks
related to the utilization of brous mineral wool (Bynum, 2001;
Papadopoulos, 2005; Al-Homoud, 2005): (a) it has very low
0892-6875/$ - see front matter 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.mineng.2010.07.015
* Corresponding author. Tel.: +30 2107722276; fax: +30 2107722168.
E-mail address: panias@metal.ntua.gr (D. Panias).
Minerals Engineering 23 (2010) 11461151
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resistance to vapour diffusion and therefore has the tendency to
increasing thermal conductivity upon vapour absorption and (b)
it has the potential to cause damage on humans health. It can irri-
tate the skin, eyes and respiratory system and therefore precau-
tions are needed during production and handling of material. The
material is reviewed by the International Agency for Research on
Cancer (IARC) as an agent belonging to group 3 not classiable
as to carcinogenicity to humans (IARC). Therefore, there is open
eld for development of a new thermal insulating material which
would potentially have the advantages of common organic and
inorganic insulating materials without having their drawbacks.
The geopolymerization technology is a low cost, green technol-
ogy (Davidovits, 2005) that can transform a variety of solid amor-
phous silicate and aluminosilicate raw materials (Panias et al.,
2007; Maragos et al., 2008; Dimas et al., 2009; Xu and van Devent-
er, 2000; Palomo et al., 1999) to useful products with high added
value (Panias et al., 2007; Maragos et al., 2008; Dimas et al.,
2009; Palomo et al., 1999; Cheng and Chiu, 2003; Wu and Sun,
2007; Pinto and Vieira, 2005). Perlite is an amorphous aluminosil-
icate volcanic glass which has the potential to be utilized as a raw
material in geopolymerization technology. Therefore, this paper
deals with the production of perlite based geopolymers which
comprise the skeleton of a newfamily of inorganic thermal insulat-
ing foamy materials that have excellent thermophysical properties,
are non-ammable and safe for humans and environment.
2. Experimental
2.1. Materials
The raw materials used for the synthesis of foamy geopolymers
were perlite, sodium hydroxide and hydrogen peroxide. The chem-
ical analysis of perlite determined by X-ray Fluorescence (XRF) is
given in Table 1 while its mineralogical analysis determined by
X-ray Diffraction (XRD) is presented in Fig. 1. Perlite is an amor-
phous volcanic glass rich in SiO
2
and Al
2
O
3
which contains some
crystalline phases as biotite, albite, quartz and calcite. The raw per-
lite used in this work was a by-product from comminution and siz-
ing operations of perlite exploitation and therefore was extremely
ne with mean particle size d
50
= 7.13 lm measured on a MAL-
VERN Laser Particle Size Analyzer. The specic gravity of perlite
measured according to the ASTM D854-06 standard using a water
pycnometer was 2.34.
The alkaline activator used for the synthesis of geopolymers
was a sodium hydroxide solution that was prepared by dissolving
anhydrous sodium hydroxide pellets (Merck Chemicals, 99.5% pur-
ity) in deionised water.
A hydrogen peroxide (H
2
O
2
) solution 30% w/w (Merck Chemi-
cals) was used as a chemical blowing agent for the foaming of
the geopolymeric pastes. H
2
O
2
is thermodynamically unstable
and therefore can be easily decomposed to water and oxygen gas
(reaction (1)) with the latter playing the role of the geopolymeric
paste blowing agent:
2H
2
O
2
!2H
2
O O
2
1
2.2. Experimental procedures
The geopolymeric viscous paste was prepared by mixing
mechanically perlite with sodium hydroxide solution. The pre-
pared paste remained at ambient temperature for 1 h and then
the necessary amount of the hydrogen peroxide (H
2
O
2
) solution
was added under mechanical mixing so that the sodium hydroxide
concentration in the aqueous phase to be 8 M and the solid to li-
quid ratio to be 1.2 g/mL. The % w/w H
2
O
2
content in the prepared
pastes was varied in-between 0.6% and 2.9%. The resulted paste
was molded in appropriate open plastic molds and was cured at
35 C for 2 h. During this period H
2
O
2
was decomposed rapidly
and the resulting oxygen blew up the paste forming the foamy
materials. Then, the curing procedure was continued at 65 C
where the materials remained for 24 h. After curing, the specimens
were de-molded and kept in a dry atmosphere. The foamy speci-
mens were prepared in two different geometries; discs with
110 mm diameter and 10 mm thickness for the measurement of
thermal conductivity and cubes with side 50 mm for the measure-
ment of compressive strength.
Table 1
Chemical analysis of perlite.
Species % w/w
SiO
2
71.58
Al
2
O
3
13.23
K
2
O 4.02
Na
2
O 3.36
CaO 2.12
Fe
2
O
3
1.83
MgO 1.04
H
2
O (chemical/combined) 2.5
Total 99.68
B
A
A
Q
C
B
B: Biotite KFeMg
2
(AlSi
3
O
10
)(OH)
2
A: Albite NaAlSi
3
O
8
Q: Quartz SiO
2
C: Calcite CaCO
3
Fig. 1. X-ray diffractogram of perlite.
V. Vaou, D. Panias / Minerals Engineering 23 (2010) 11461151 1147
2.3. Analysis and tests
The apparent density (q) of the foamy geopolymers was deter-
mined by measuring the weight of specimens with a precision bal-
ance as well as their dimensions with a precision electronic
calliper. The density (d) of the geopolymeric matrix was measured
according to the ASTM D854-06 standard using a water pycnome-
ter. The % cell volume (C) of the foamy materials was determined
according to the following formula:
C
1 q 100
d
2
The thermal conductivity was measured with a thermal conduc-
tivity analyser (Mathis TCi, SETARAM) utilizing the modied tran-
sient plane source technique. The compressive strength was
measured on a testing machine of the Structural Behavior Engineer-
ing Laboratories Inc. (PLT-10 model). For the determination of the
material properties two specimens were always tested and the
average value of measurements was reported as the result. Finally,
the cell structure was examined by scanning electron microscopy
(SEM) on a JOEL JSM-type scanning electron microscope.
3. Results and discussion
3.1. Properties of the foamy materials
The effect of H
2
O
2
content in the geopolymeric paste on the
apparent density as well as % cell volume of foamy materials is
shown in Fig. 2. Two regions can be seen; (a) the region I in-be-
tween 0.7% and 2% w/w H
2
O
2
where the apparent density de-
creases sharply from 665 kg/m
3
to 335 kg/m
3
as the H
2
O
2
content in the geopolymeric paste increases accompanied by a
substantial increase of the cell volume from almost 7487% and
(b) the region II for H
2
O
2
content higher than 2% w/w where the
change of the apparent density as well as the % cell volume is prac-
tically limited and the foamy materials tend to have an apparent
density a little bit higher or lower than 300 kg/m
3
and a cell vol-
ume varied in-between 87% and 89%. This behaviour can be under-
stood in view of the foaming mechanism of the geopolymeric
paste. The decomposition of hydrogen peroxide liberates oxygen
creating initially very small bubbles inside the mass of the very vis-
cous paste which behaves as a non-Newtonian plastic or pseudo-
plastic uid. The pressure exerted on the bubbles wall plays the
role of the shear stress for the viscous paste which is deformed
causing the bubbles expansion and the foaming of the paste. The
bubbles expansion causes a decrease of the oxygen pressure under
constant temperature eliminating gradually the shear stress and
therefore stopping the bubbles expansion and the pastes foaming.
When the oxygen volume per paste volume is low enough (the
case of low H
2
O
2
content), the spherical bubbles are discernible
and they have low population density in the geopolymeric paste.
As the H
2
O
2
content increases, the bubbles population density in-
creases as well as the amount of oxygen in each bubble do due to
the increased local oxygen concentration. Therefore, the bubble
size increases, the thickness of the cells as well as the apparent
density of foams decrease and the cell volume increases (region I
linear part with high gradient). When the oxygen volume per
paste volume exceeds a threshold, the bubbles population density
and the amount of oxygen per bubble increase substantially result-
ing the aggregation of a number of cells creating a network of cells
partially open to environment and thus causing marginal expan-
sion and marginal increase to the cell size (region II linear part
with small gradient).
The microstructure of foamy materials is presented in Fig. 3.
The cells are normally closed and almost spherical when the % con-
tent of H
2
O
2
in the paste is low. Aggregation among cells takes
place as the % content of H
2
O
2
increases changing the cells geo-
metrical shape from spherical to oval, creating a network of inter-
connecting cells and affecting the mean cell size as is seen in Figs. 3
and 4.
The mean cell size is 700 lm at the lowest studied H
2
O
2
content
of 0.7% increasing almost linearly with the H
2
O
2
content and reach-
ing at the value of 1.9 mm at 2.02% H
2
O
2
in the geopolymeric paste.
Further increase of H
2
O
2
content up to the highest studied value of
2.95% causes marginal changes on cell size, which reaches the va-
lue of 2.08 mm, explaining thus the limited increase of cell volume
as well as the decrease of apparent density (Fig. 2) of foamy mate-
rials in the same range of % H
2
O
2
content.
The thermal conductivity of foamy materials is shown in Fig. 5.
Thermal conductivity follows identical trend with apparent density
decreasing substantially from 0.053 W/m K to 0.03 W/m K as the
H
2
O
2
content ranging in-between 0.7% and 2.02%. Further increase
of the H
2
O
2
content in the geopolymeric paste to the studied value
of 2.95% w/w has not a measurable effect on the thermal conduc-
tivity value. The results showed that the thermal conductivity of
foamy geopolymers is correlated to their cellular structure and a
substantial decrease of the thermal conductivity value can be
achieved by controlling appropriately the cells type, size, shape
and volume. The results are in good agreement with the state-of-
the-art on thermal insulation foamed plastics where the thermal
conductivity is correlated rstly to the thermal conductivity of
the lling gas followed by the apparent density of foams and then
the morphology of the cellular structure (Weber et al., 2005).
The compressive strength of foamy materials is shown in Fig. 6.
The fracture of materials resembles the behaviour of rocks for H
2
O
2
content in the geopolymeric paste higher than 1.58%. In this case
the materials have almost the same compressive strength of
780 kPa. For H
2
O
2
content lower than 1.58%, the materials have
more plasticity due to incomplete geopolymerization because the
network of small and closed cells hinders the water removal during
the curing period. Therefore, the incomplete geopolymerized
foamed materials have compressive strength ranging in-between
250 and 780 kPa.
3.2. Comparison with the other current state-of-the-art insulating
materials
A comparison among the state-of-the-art commercially avail-
able organic and inorganic insulating materials as well as of the
best foamy perlite geopolymer produced in this work (with
72
74
76
78
80
82
84
86
88
90
0
100
200
300
400
500
600
700
0 0.5 1 1.5 2 2.5 3 3.5
%

C
e
l
l

V
o
l
u
m
e
A
p
p
a
r
e
n
t

d
e
n
s
i
t
y

o
f

f
o
a
m
y

m
a
t
e
r
i
a
l
s
,

K
g
/
m
3
2 2
content in geopolymeric paste, % w/w
Apparent Density
Cell Volume
o H
Fig. 2. Apparent density and % cell volume of foamy materials as a function of % w/w
H
2
O
2
content in the geopolymeric paste.
1148 V. Vaou, D. Panias / Minerals Engineering 23 (2010) 11461151
2.9% w/w H
2
O
2
in the geopolymeric paste) is shown in Table 2. The
foamy perlite geopolymer is a very good thermal insulating mate-
rial. Its thermal conductivity value of 0.03 W/m K is directly com-
parable with the lowest ones of the organic materials (XPS and
EPS) as well as of inorganic materials (glass and mineral wool).
The maximum application temperature of foamy perlite geopoly-
mer is 700 C which is substantially higher than the ones of organic
materials, higher than the one of glass wool and directly compara-
ble of the one of mineral wool. The foamy perlite geopolymer does
not melt in the temperature region in-between 700 and 1000 C
but it softens due to the glassy nature of perlite. The perlitic water
trapped in the structure of perlite particles vaporizes and therefore
expand the foamy geopolymer decreasing its apparent density
from 290 kg/m
3
to 160 kg/m
3
without affecting the value of ther-
mal conductivity. The geometrical features (shape and dimensions)
of foamy geopolymers change during the softening procedure and
for this reason the temperature of 700 C is chosen as the maxi-
mum application temperature.
The 100% inorganic nature of foamy perlite geopolymer renders
it totally non-combustible categorizing it in the Fire Class A1 in
accordance to the standard DIN4102. The foamy perlite geopoly-
mer has superior re resistant properties in comparison to the
other common organic and inorganic insulating materials shown
in Table 2. The commercial inorganic insulating materials such as
0.7 % w/w H
2
O
2
1.58 % w/w H
2
O
2
2.02 % w/w H
2
O
2
2.95 % w/w H
2
O
2
Fig. 3. SEM photos of foamy materials prepared with different % w/w H
2
O
2
content in the geopolymeric paste.
0
500
1000
1500
2000
2500
0 0.5 1 1.5 2 2.5 3 3.5
M
e
a
n

c
e
l
l

s
i
z
e
,

m
H
2
O
2
in geopolymeric paste, % w/w
Fig. 4. Mean cell size as a function % w/w H
2
O
2
content in the geopolymeric paste.
0.000
0.010
0.020
0.030
0.040
0.050
0.060
0 0.5 1 1.5 2 2.5 3 3.5
T
h
e
r
m
a
l

c
o
n
d
u
c
t
i
v
i
t
y
,

W
/
m
.
K
H
2
O
2
content in geopolymeric paste , % w/w
Fig. 5. Thermal conductivity of foamy materials as function % w/w H
2
O
2
content in
the geopolymeric paste.
0
100
200
300
400
500
600
700
800
900
0 0.5 1 1.5 2 2.5 3 3.5
C
o
m
p
r
e
s
s
i
v
e

s
t
r
e
n
g
t
h
,

k
P
a
H
2
O
2
in geopolymeric paste, % w/w
Fig. 6. Compressive strength of foamy materials as function % w/w H
2
O
2
content in
the geopolymeric paste.
V. Vaou, D. Panias / Minerals Engineering 23 (2010) 11461151 1149
mineral and glass wool are often characterized in the A2 Fire Class
(about 98% non-combustible) because they contain a combustible
organic binder which binds the inorganic bres creating the mar-
ketable products in the form of panels or felts.
The fractural behaviour of foamy perlite geopolymers resembles
the one of rocks and is totally different from the behaviour of the
other commercial inorganic and organic insulating materials
shown in Table 2. The foamy geopolymer has not plasticity or elas-
ticity and has enough high compressive strength for the practical
application of buildings insulation. In general, it has superior
mechanical properties in relation to the other common insulating
materials.
The relative high value of apparent density is the most impor-
tant drawback of foamy perlite geopolymer in relation to the other
common insulating materials. The achieved value of 290 kg/m
3
is
almost 1.6 and 3.6 times higher than the corresponding ones of
mineral wool and extruded polystyrene which are commonly used
for buildings insulation. Improving apparent density is a target of
great importance for the commercial application of foamy perlite
geopolymers. This target could be achieved by the application of
one of the three following actions or by the synergetic effect of
all of them:
(a) Foaming of geopolymeric paste by blowing air under con-
trolled pressure and volumetric ow rate (mechanical foam-
ing) instead of blowing by chemical means as it was applied
in this work. Mechanical foaming can achieve better cells
structure and % cell volume higher than 90% decreasing the
apparent density of foamy materials up to 150200 kg/m
3
.
(b) Use of expanded instead of non-expanded perlite as a raw
material for synthesis of geopolymers. Taking into account
that the bulk density of expanded perlite is in-between 30
and 150 kg/m
3
while the bulk density of non-expanded per-
lite is about 1100 kg/m
3
, it could be assumed that foamy
geopolymers based on expanded perlite would have appar-
ent density in-between 20 and 100 kg/m
3
which is a value
directly comparable with the apparent densities of the com-
mon commercial insulating materials. Although this work
did not study the expanded perlite as a raw material for geo-
polymerization, the thermal tests for determination of the
maximum application temperature of foamy perlite geo-
polymer showed that at temperatures in-between 700 and
1000 C the apparent density of foamy materials decreased
to a value of 160 kg/m
3
due to incomplete perlite expansion.
Therefore, this result offer indirect evidence that the above
stated assumption is not an illusion and could be a good esti-
mate for the apparent density of foamy expanded perlite
geopolymers.
(c) The temperature at which the green foamy perlite geopoly-
mers are cured can affect the apparent density of nal mate-
rials. As is seen in Fig. 7, 810% of the weight of foamy
materials is physically adsorbed water which can be easily
removed at curing temperatures around 100 C decreasing
the apparent density of materials.
Finally, water absorption measured by the resistant to vapour
diffusion factor and/or humidity assimilation rate is a very impor-
tant physical property that can affect the thermal conductivity of
insulating materials. The foamy perlite geopolymers, especially
the ones that have been produced with high H
2
O
2
content in the
geopolymeric paste, can absorb water and have low resistant to va-
pour diffusion factor, because they are consisting of networks of
interconnecting cells some of which are partially open to the envi-
ronment, increasing their thermal conductivity value. This is the
other drawback of the foamy perlite geopolymer produced in this
work. To avoid this drawback, the foamy perlite geopolymer has
to be provided, where necessary, with a very thin geopolymeric
surface cover with very low permeability (Maragos et al., 2008).
Table 2
Typical values of the basic thermophysical properties of common insulating materials.
Material Glass
wool
Mineral wool Extruded polystyrene,
XPS
Expanded polystyrene,
EPS
Foamy perlite
geopolymer
Apparent density, kg/m
3
13100 30180 2080 1850 290
Thermal conductivity, W/m K 0.03
0.045
0.0330.045 0.0250.035 0.0290.041 0.03
Maximum application temperature, C 500 750 75 80 700
Fire Class A1A2 A1A2 B1B2 B1B2 A1
Compressive strength at 10% deformation,
kPa
16 (1) 0.0169 (1), (2),
(3)
100700 (4) 70450 (5), (6), (7) 780
a
The most values have been taken from Papadopoulos (2005).
(1) National Insulation Co.
(2) Buska and Maciulaitis (2007).
(3) Industrial Insulation Group.
(4) Extruded Polystyrene Foam Association.
(5) EPS Molders Association.
(6) Desjarlais and Zarr (2002).
(7) Quality Foam.
a
The material is fractured at 2% deformation.
-3
-2
-1
0
1
2
3
4
5
6
-20
-18
-16
-14
-12
-10
-8
-6
-4
-2
0
0 100 200 300 400 500 600 700 800 900
H
e
a
t

F
l
o
w
,

V
%

W
e
i
g
h
t

L
o
s
s
Temperature,
o
C
E
x
o
Fig. 7. Typical TG/DTA curves for foamy perlite materials which have been
synthesized with 2.98% w/w H
2
O
2
content in the geopolymeric paste.
1150 V. Vaou, D. Panias / Minerals Engineering 23 (2010) 11461151
4. Conclusions
Foamy geopolymers from non-expanded perlite proved to be
very good thermal insulating materials. In comparison with the
commercial organic (expanded and extruded polystyrene) and
inorganic (glass and stone wool) thermal insulating materials,
the foamy geopolymers from perlite have (a) almost similar ther-
mal conductivity (0.03 W/m K); (b) superior compressive strength
(780 kPa at 2% deformation) and a fracture behaviour resembling
the one of rocks; (c) superior re resistant properties (100% non-
combustible) categorizing them in the Fire Class A1 according to
DIN4102; (d) superior maximum application temperature
(700 C) only comparable with the one of mineral wool, which ren-
der the material proper not only for buildings thermal insulation
but also for industrial insulation applications where high temper-
atures occur.
At the current stage of development, foamy geopolymers from
non-expanded perlite have the two following drawbacks: (a) rela-
tively high apparent density (290 kg/m
3
) and (b) high water
absorption capacity. The most promising way to decrease the
apparent density at a level comparable to the ones of commercial
organic and inorganic thermal insulating materials is the synthesis
of foamy geopolymers utilizing (a) expanded instead of non-ex-
panded perlite as a solid raw material and (b) mechanical foaming
of geopolymeric paste by blowing air under controlled pressure
and volumetric ow rate. Finally, an effective way to increase the
resistant to vapour diffusion factor is to cover the surface of foamy
geopolymers with a thin layer from a compact geopolymer with
low permeability which is a practice always applied to materials
with open or partially open cellular structure.
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